CN115532229A - Preparation of magnetic adsorbent material and application of bacterium carrier construction in removing aflatoxin - Google Patents
Preparation of magnetic adsorbent material and application of bacterium carrier construction in removing aflatoxin Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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Abstract
The invention belongs to the technical field of adsorbent materials, and particularly relates to a preparation method of a magnetic adsorbent material and application of a bacterial carrier in construction and removal of aflatoxin, wherein the preparation method comprises the following steps: crushing the adsorbent by using a wall breaking machine to obtain adsorbent particles, and sieving the adsorbent particles by using a 200-mesh sieve; weighing ferrous sulfate and ferric chloride, dissolving the ferrous sulfate and ferric chloride in deionized water, adding the prepared adsorbent particles, stirring at a high speed by using a magnetic stirrer, and dripping sodium hydroxide solution under high-speed stirring; aging the obtained mixture in a water bath at 100 ℃, and cooling; washing the product, drying and sieving to obtain the magnetic adsorbent which is the required magnetic adsorbent material. The preparation method of the magnetic adsorbent material provided by the invention is scientific and reasonable in design, can effectively remove aflatoxin AFB1 in bulk grains, and can further improve the removal effect of aflatoxin AFB1 after the magnetic adsorbent material is combined with a bacillus subtilis strain screened in a laboratory to form a thallus compound.
Description
Technical Field
The invention belongs to the technical field of adsorbent materials, and particularly relates to a preparation method of a magnetic adsorbent material and application of a bacterial carrier in construction and removal of aflatoxin.
Background
In recent years, the safety of livestock products is gradually concerned by consumers, and the safety of livestock products is directly influenced by the safety of feed. Contamination of feed with mycotoxins can result in a reduction in its nutritional value, cause disease in animals, and harm human health directly or indirectly. Aflatoxins are a class of biotoxins produced by aspergillus flavus that are toxic to humans and livestock, causing significant losses to the livestock breeding industry. Aflatoxins are derivatives of dihydrofurocoumarins, a toxic metabolite of fungi, and are present in natural soils and rotten plants. The probability of aflatoxin in the environment with the temperature of 25-300 ℃ and the relative humidity of 80-90% is the highest for the feed and the feed raw materials. The aflatoxin mould is a storage bacterium which is widely distributed in nature and can not be seen by naked eyes, and the generation of the aflatoxin mould is still a natural threat for the safety of livestock and poultry feed and feed raw materials. Aflatoxin, which is the most liable to contaminate grain and oil products, such as peanut, corn, rice, soybean, wheat, etc., is one of mycotoxins that is the most serious harm to human health, and has attracted extensive attention.
Physical detoxification method the physical method for aflatoxin detoxification treatment comprises the following steps: removing mildew, ultraviolet irradiation, air drying, degerming (for detoxicating mildewed semen Maydis), etc.; however, the above method is not feasible for feed production enterprises and livestock and poultry breeding industries because it is very difficult to detoxify large batches of feed or raw materials by the above physical methods.
At present, a feasible detoxification method is an adsorption method, i.e. a method for detoxification by adding mycotoxin adsorbent into feed. Is simple and effective for the feed production and the detoxification method of the adsorbent in livestock and poultry breeding industry. The selection of the adsorbent is based on the principle of strong adsorption capacity, high efficiency, practicality, low cost and no negative influence. The feed capable of adsorbing mycotoxin is mixed into a feed product, and the aim is to adsorb aflatoxin in the digestive tract of animals and prevent the organisms from absorbing the toxin, so that the harm and residue of the toxin to the animals are reduced, and the detoxification effect is achieved. The common adsorbent comprises zeolite, bentonite, montmorillonite, active carbon and the like, has stable properties, is insoluble in water, cannot be absorbed by animals, and has strong adsorption effect.
However, with the development of fermentation technology, the adsorption capacity of the traditional adsorbent can not meet the requirement, and the traditional adsorbent needs to be improved to obtain better adsorption capacity so as to efficiently adsorb and remove aflatoxin in the feed in a fermentation tank.
Disclosure of Invention
The present invention is directed to overcoming the above problems in the conventional art, and provides a method for preparing a magnetic adsorbent material, comprising the steps of:
1) Crushing the activated carbon for 20-40 min by using a wall breaking machine at normal temperature to obtain activated carbon particles, and sieving the activated carbon particles with a 200-mesh sieve for later use;
2) Weighing ferrous sulfate and ferric chloride, dissolving the ferrous sulfate and ferric chloride in 250ml of deionized water, adding the prepared activated carbon particles, stirring the mixture for 20 to 40min at a high speed by using a magnetic stirrer, and dropwise adding 50ml of sodium hydroxide solution under high-speed stirring to obtain a mixture;
3) Aging the obtained mixture in a water bath at 100 ℃ for 3-5 h, and cooling to normal temperature;
4) Repeatedly washing the product obtained in the step 3) by using deionized water, carrying out ultrasonic oscillation in absolute ethyl alcohol for 10-30 min, then placing the product in a drying oven for drying for 3-5 h, and sieving the product by using a 200-mesh sieve to obtain the magnetic activated carbon, namely the required magnetic adsorbent material.
Further, in the preparation method, step 1), the activated carbon is broken for 30min by using a wall breaking machine.
Further, in the above preparation method, step 1), the adsorbent is activated carbon.
Further, in the preparation method, in the step 2), the mass ratio of the ferrous sulfate, the ferric chloride and the activated carbon particles is 1-2: 1 to 2:1.
further, the preparation method as described above, step 2). The concentration of sodium hydroxide was 5mol/L.
Further, in the above-mentioned preparation method, step 3), the resulting mixture was aged in a water bath at 100 ℃ for 4 hours and cooled to normal temperature.
Further, in the preparation method as described above, in step 4), the product of step 3) is repeatedly washed with deionized water, and is subjected to ultrasonic oscillation in absolute ethyl alcohol for 20min, and then is placed in a drying oven for drying for 4h.
The invention also provides a magnetic adsorbent material prepared by the preparation method.
The invention also provides a bacterial compound which is formed by combining the magnetic adsorbent material and the bacillus strain, wherein the bacillus strain is the bacillus strain WTX1 which is separated from the yak dung on the Qinghai-Tibet plateau in a laboratory and has AFB1 degradation rate of 83.5%, and the AFB1 concentration is 10 mug/mL of culture solution. The specific method comprises the following steps: inoculating 13% of the inoculum size into the activated bacillus strain WTX1, fixing for 18h at the temperature of 37 ℃ at the rotating speed of 120r/min, taking the bacillus strain WTX, centrifuging for 4min at the rotating speed of 3000r/min, coating the supernatant on a beef extract peptone culture medium, performing blank control with free bacteria, and determining the fixing rate of the carrier on the microorganisms.
The invention also provides an application, and particularly the magnetic adsorbent material and the thallus compound can be used for removing aflatoxin.
The beneficial effects of the invention are:
the preparation method of the magnetic adsorbent material provided by the invention is scientific and reasonable in design, can effectively remove aflatoxin AFB1 in a large amount of grains, and can further improve the removal effect of aflatoxin AFB1 after the magnetic adsorbent material is combined with a bacillus subtilis strain screened in a laboratory to form a thallus compound.
Of course, it is not necessary for any one product that embodies the invention to achieve all of the above advantages simultaneously.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a sewage simulation standard curve diagram of methylene blue;
FIG. 2 is an adsorption capacity diagram for simulated wastewater treatment in example 1 and comparative examples 1 to 3;
FIG. 3 is an adsorption energy diagram for aflatoxin AFB1 in example 1 and comparative examples 1-3;
FIG. 4 is a Fourier Infrared test chart of examples 1-2.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of a magnetic adsorbent material comprises the following steps:
crushing the activated carbon for 30min by using a wall breaking machine at normal temperature to obtain activated carbon particles, and sieving the activated carbon particles with a 200-mesh sieve for later use. Weighing 9.75g of ferrous sulfate and 9.45g of ferric chloride, dissolving in 250ml of deionized water, adding 8.25g of prepared activated carbon particles, stirring at high speed for 30min by using a magnetic stirrer, dropwise adding a sodium hydroxide (50ml, 5 mol/L) solution under high-speed stirring, aging the obtained mixture in a water bath at 100 ℃ for 4h, cooling to normal temperature, repeatedly washing the product by using deionized water, carrying out ultrasonic oscillation in absolute ethyl alcohol for 20min, drying in a drying box for 4h, and sieving with a 200-mesh sieve twice to obtain the magnetic activated carbon.
Example 2
An antimicrobial composition comprising the steps of:
crushing the activated carbon for 30min by using a wall breaking machine at normal temperature to obtain activated carbon particles, and sieving the activated carbon particles with a 200-mesh sieve for later use. Weighing 9.75g of ferrous sulfate and 9.45g of ferric chloride, dissolving in 250ml of deionized water, adding 8.25g of prepared activated carbon particles, stirring at high speed for 30min by using a magnetic stirrer, dropwise adding a sodium hydroxide (50ml, 5 mol/L) solution under high-speed stirring, aging the obtained mixture in a water bath at 100 ℃ for 4h, cooling to normal temperature, repeatedly washing the product by using deionized water, carrying out ultrasonic oscillation in absolute ethyl alcohol for 20min, drying in a drying box for 4h, and sieving with a 200-mesh sieve twice to obtain the magnetic activated carbon.
Magnetic activated carbon is combined with the bacillus subtilis strain to prepare a thallus compound. Specifically, activated bacillus strain WTX1 (culture solution with the degradation rate of 83.5% and the AFB1 concentration of 10 mu g/mL) is inoculated in 13% of inoculum size, the strain is fixed for 18 hours at the temperature of 37 ℃ and the rotating speed of 120r/min, then the strain is taken out at 3000r/min and centrifuged for 4 minutes, the supernatant is coated on a beef extract peptone culture medium, a blank control is carried out on the culture medium and free bacteria, and the fixing rate of the carrier to microorganisms is measured.
Comparative example 1
A preparation method of a magnetic adsorbent material comprises the following steps:
crushing bentonite for 30min by using a wall breaking machine at normal temperature to obtain bentonite particles, and sieving the bentonite particles with a 200-mesh sieve for later use. Weighing 9.75g of ferrous sulfate and 9.45g of ferric chloride, dissolving in 250ml of deionized water, adding 8.25g of prepared bentonite particles, stirring at high speed for 30min by using a magnetic stirrer, dropwise adding a sodium hydroxide (50ml, 5 mol/L) solution under high-speed stirring, aging the obtained mixture in a water bath at 100 ℃ for 4h, cooling to normal temperature, repeatedly washing the product by using deionized water, carrying out ultrasonic oscillation in absolute ethyl alcohol for 20min, drying in a drying box for 4h, and sieving with a 200-mesh sieve for the second time to obtain the magnetic bentonite.
Comparative example 2
A preparation method of a magnetic adsorbent material comprises the following steps:
crushing the straw biochar for 30min by using a wall breaking machine at normal temperature to obtain straw biochar particles, and sieving the straw biochar particles with a 200-mesh sieve for later use. Weighing 9.75g of ferrous sulfate and 9.45g of ferric chloride, dissolving in 250ml of deionized water, adding 8.25g of prepared straw biochar particles, stirring at high speed for 30min by using a magnetic stirrer, dropwise adding a sodium hydroxide (50ml, 5 mol/L) solution under high-speed stirring, aging the obtained mixture in a water bath at 100 ℃ for 4h, cooling to normal temperature, repeatedly washing the product by using deionized water, carrying out ultrasonic oscillation in absolute ethyl alcohol for 20min, then placing in a drying box for drying for 4h, and sieving with a 200-mesh sieve twice to obtain the magnetic straw biochar.
Comparative example 3
A preparation method of a magnetic adsorbent material comprises the following steps:
crushing pine charcoal with a wall breaking machine at room temperature for 30min to obtain pine charcoal granules, and sieving with a 200-mesh sieve. Weighing 9.75g of ferrous sulfate and 9.45g of ferric chloride, dissolving in 250ml of deionized water, adding 8.25g of prepared pine charcoal particles, stirring at high speed for 30min by using a magnetic stirrer, dripping sodium hydroxide (50ml, 5 mol/L) solution under high-speed stirring, aging the obtained mixture in a water bath at 100 ℃ for 4h, cooling to normal temperature, repeatedly washing the product by using deionized water, carrying out ultrasonic oscillation in absolute ethyl alcohol for 20min, drying in a drying box for 4h, and sieving with a 200-mesh sieve for the second time to obtain the magnetic pine charcoal.
The magnetic adsorbent materials obtained in example 1 and comparative examples 1 to 3 are used as samples, and the adsorption performance of simulated sewage is characterized as follows:
first, a methylene blue wastewater simulation standard curve is prepared, as shown in FIG. 1.
Then, an adsorption performance test simulating sewage treatment was performed, and the results are shown in fig. 2.
The simulated sewage treatment proves that the adsorbent has remarkable adsorption performance, the specific magnetic saturation intensity of the magnetic carbon is further measured, and the measurement results are shown in Table 1
TABLE 1
| Name (R) | Specific saturation magnetization (emu/mg) | BET specific surface area (m) 2 /g) |
| |
0 | 441.32 |
| Magnetic activated carbon | 30.13 | 272.71 |
| |
0 | 48.41 |
| Magnetic bentonite | 28.28 | 62.28 |
| |
0 | 174.32 |
| Magnetic pine charcoal | 21.99 | 31.83 |
| |
0 | 8.96 |
| Magnetic straw biochar | 29.26 | 39.86 |
The magnetic adsorbent materials obtained in example 1 and comparative examples 1 to 3 were used as samples to test the adsorption capacity of aflatoxin AFB1, and the results are shown in FIG. 3. The obtained magnetic activated carbon has the strongest adsorption capacity and accords with an adsorption kinetic equation.
In example 2, the magnetic activated carbon was further bound to Bacillus subtilis to form a cell complex, and the surface of the magnetic activated carbon was analyzed for functional groups by Fourier infrared analysis, and the results are shown in FIG. 4.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (10)
1. The preparation method of the magnetic adsorbent material is characterized by comprising the following steps:
1) Crushing the adsorbent for 20-40 min by using a wall breaking machine at normal temperature to obtain adsorbent particles, and sieving the adsorbent particles by using a 200-mesh sieve for later use;
2) Weighing ferrous sulfate and ferric chloride, dissolving the ferrous sulfate and ferric chloride in 250ml of deionized water, adding the prepared adsorbent particles, stirring at high speed for 20-40 min by using a magnetic stirrer, and dropwise adding 50ml of sodium hydroxide solution under high-speed stirring to obtain a mixture;
3) Aging the obtained mixture in a water bath at 100 ℃ for 3-5 h, and cooling to normal temperature;
4) Repeatedly washing the product obtained in the step 3) by using deionized water, carrying out ultrasonic oscillation in absolute ethyl alcohol for 10-30 min, then placing the product in a drying oven for drying for 3-5 h, and sieving the product by using a 200-mesh sieve to obtain the magnetic adsorbent, namely the required magnetic adsorbent material.
2. The method of claim 1, wherein: in the step 1), a wall breaking machine is adopted to break the adsorbent for 30min.
3. The method of claim 1, wherein: in the step 1), the adsorbent is activated carbon.
4. The method of claim 1, wherein: in the step 2), the mass ratio of ferrous sulfate, ferric chloride and adsorbent particles is 1-2: 1 to 2:1.
5. the method of claim 1, wherein: in step 2). The concentration of sodium hydroxide was 5mol/L.
6. The production method according to claim 1, characterized in that: in the step 3), the obtained mixture is aged in a water bath at 100 ℃ for 4 hours and cooled to the normal temperature.
7. The method of claim 1, wherein: in the step 4), repeatedly washing the product in the step 3) by using deionized water, carrying out ultrasonic oscillation in absolute ethyl alcohol for 20min, and then placing in a drying oven for drying for 4h.
8. A magnetic adsorbent material produced by the production method according to any one of claims 1 to 7.
9. A bacterial complex formed by combining the magnetic adsorbent material of claim 8 with a bacillus strain, which is a bacillus strain WTX1 with AFB1 degradation rate of 83.5% isolated from yak dung in Qinghai-Tibet plateau in laboratory, wherein the concentration of AFB1 is 10 μ g/mL of culture solution.
10. The magnetic adsorbent material according to claim 8 or the bacterial compound according to claim 9 for use in aflatoxin removal.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116239180A (en) * | 2023-03-14 | 2023-06-09 | 河南工业大学 | Removal of aflatoxin B by ferromagnetic porous carbon material 1 Is a method of (2) |
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